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New Materials for Strontium Removal from Nuclear Waste Streams New Materials for Strontium Removal from Nuclear Waste Streams by Savvaki Neoklis Savva Supervisor: Dr Joseph A. Hriljac A thesis submitted to The University of Birmingham for the degree of Doctor of Philosophy The School of Chemistry College of Engineering and Physical Sciences University of Birmingham September 2015 University of Birmingham Research Archive e-theses repository This unpublished thesis/dissertation is copyright of the author and/or third parties. The intellectual property rights of the author or third parties in respect of this work are as defined by The Copyright Designs and Patents Act 1988 or as modified by any successor legislation. Any use made of information contained in this thesis/dissertation must be in accordance with that legislation and must be properly acknowledged. Further distribution or reproduction in any format is prohibited without the permission of the copyright holder. Abstract The primary aim of this project is to investigate potential new materials for application in ion exchange processes to remove 90Sr from nuclear waste streams. This work can be broadly split in to two sections, work on attempts to synthesise new materials and work to investigate ion exchange properties of two recently prepared materials AV-7, a synthetic analogue of tin- kostylvite and AV-3, a synthetic analogue of petarasite. Synthesis on new materials was focused on metal silicate materials, in particular titanium, zirconium and tin silicates containing exchangeable group I and II cations. These synthesis attempts initially were focus on targeted mineral phases such as noonkanbahite, BaKNaTi2(Si4O12)O2, followed by a series of brief surveys examining the effects of various changes to precursor gels such as concentration of bases such as NaOH, metal to silicon ratios and the presence of mineralizing agents such as sodium fluoride. The synthesis of two synthetic mineral phases potentially interesting for ion exchange is also reported here, titanite and fresnoite. Ion exchange studies focused mainly on AV-7 and AV-3 but also included well known ion exchange materials for comparison such as clinoptilolite and Nb-doped crystalline silicotitanate and brief investigations in to the ion exchange of fresnoite and titanite. Ion exchange was followed using X-Ray fluorescence, ion chromatography and radioactive 85Sr exchanges measured using scintillation counters. Acknowledgements I would firstly like to thank my supervisor Dr Joe Hriljac for all his support throughout this PhD project and all its difficulties. Thanks also to those at the NNL who helped with this work in particular my NNL supervisor Dr. Zoe Maher for some valuable guidance but also to Dr. Scott Owns for useful discussions. Financial sponsorship from the School of Chemistry, University of Birmingham and the NNL is also gratefully acknowledged. A special thanks to past and present members of the Hriljac group, Tom Carey for help with my crystallography problems and George and Geoff for the time we spent in Boston. A special thanks to Evin who has been an incredible help throughout my time here. I would also like to thank all those from the 5th floor of chemistry who helped in innumerable ways over the course of my work, from useful discussions over cups of tea to blowing of steam bouldering. A great thanks also to Dr Jackie Deans whose technical support has been a great help to me and everyone on floor five. Finally I’d like to thank Katrina whose love, patience and support have helped with the hardest part of this work, the writing of it. Contents Chapter 1 – Introduction…………………………………………………………………....….1 1.1 Background ……………………………………………………………………………..1 1.2 Ion exchange ..................................................................................................................... 3 1.3 Inorganic ion exchangers .................................................................................................. 5 1.3-1 Natural inorganic ion exchangers .............................................................................. 5 1.3-2 Synthetic ion exchangers ........................................................................................... 9 1.4 Potential materials for ion exchange – scope of this work ............................................. 16 Chapter 2 - Experimental……………………………………………………………………..17 2.1 Synthesis techniques ........................................................................................................... 22 2.1-1 Solid state synthesis ..................................................................................................... 22 2.1-2 Sol-gel synthesis .......................................................................................................... 22 2.1-3 Hydrothermal synthesis ............................................................................................... 22 2.1-4 Microwave synthesis ................................................................................................... 23 2.2 Characterisation techniques ................................................................................................ 24 2.2-1 Fundamentals of crystallography and diffraction ........................................................ 24 2.2-2 Neutron diffraction ...................................................................................................... 33 2.2-3 Rietveld refinement ..................................................................................................... 35 2.2-4 X-ray fluorescence spectrometry ................................................................................. 39 2.2-5 Scanning electron microscopy (SEM) ......................................................................... 44 2.2-6 Ion chromatography ..................................................................................................... 46 2.2-7 Radiotracer studies ...................................................................................................... 48 Chapter 3 - Titanosilicates and zirconosilicates………………………………………………45 3.1 Introduction ........................................................................................................................ 51 3.2 Experimental ....................................................................................................................... 53 3.2-1 Noonkanbahite & related phases synthesis gels .......................................................... 53 3.2-2 Titanite synthesis gels .................................................................................................. 55 3.2-3 Zirconosilicate synthesis gels ...................................................................................... 56 3.2-4 Ion exchanges .............................................................................................................. 58 3.3 Results and discussion ........................................................................................................ 58 3.2-1 Noonkanbahite and related phases .............................................................................. 58 3.2-2 Titanite ......................................................................................................................... 62 3.3-3 fresnoite ....................................................................................................................... 68 3.3-4 Zirconosilicate synthesis ............................................................................................. 72 3.3-4a Synthesis and characterisation of synthetic petarasite (AV-3) .............................. 75 3.4 Conclusions ........................................................................................................................ 94 Chapter 4 - Tin silicates ……………………………………………………………………...89 4.1 Introduction ........................................................................................................................ 95 4.2 Experimental ....................................................................................................................... 96 4.2-1 Hydrothermal SnO2-SiO2-NaOH synthesis survey ..................................................... 96 II 4.2-2 Microwave Tin survey ............................................................................................... 97 4.2-3 AV-7 - synthetic tin kostylvite .................................................................................... 98 4.2-4 Ion exchanges .............................................................................................................. 98 4.2-4a Bulk ion exchange .................................................................................................. 98 4.2-4b Low concentration ion exchange ........................................................................... 99 4.2-4c Fused bead XRF ..................................................................................................... 99 4.3 Results and discussion ...................................................................................................... 100 4.3-1 SnO2-SiO2-NaOH synthesis survey ........................................................................... 100 4.3-2 Microwave TinII survey ............................................................................................. 101 4.3-3 AV-7 - synthetic tin kostylvite ............................................................................... 109 4.3-4 Ion Exchanges .......................................................................................................
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